EP1630249A2 - Procédé de dépôt en phase vapeur de nitrure de silicium. - Google Patents

Procédé de dépôt en phase vapeur de nitrure de silicium. Download PDF

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Publication number
EP1630249A2
EP1630249A2 EP05018682A EP05018682A EP1630249A2 EP 1630249 A2 EP1630249 A2 EP 1630249A2 EP 05018682 A EP05018682 A EP 05018682A EP 05018682 A EP05018682 A EP 05018682A EP 1630249 A2 EP1630249 A2 EP 1630249A2
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European Patent Office
Prior art keywords
substrate
silicon nitride
zone
ammonia
iii
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EP05018682A
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German (de)
English (en)
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EP1630249A3 (fr
Inventor
Arthur Kenneth Hochberg
Kirk Scott Cuthill
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Air Products and Chemicals Inc
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Air Products and Chemicals Inc
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Publication of EP1630249A2 publication Critical patent/EP1630249A2/fr
Publication of EP1630249A3 publication Critical patent/EP1630249A3/fr
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
    • H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
    • H01L21/0217—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material being a silicon nitride not containing oxygen, e.g. SixNy or SixByNz
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/34—Nitrides
    • C23C16/345—Silicon nitride
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
    • H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
    • H01L21/02211—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound being a silane, e.g. disilane, methylsilane or chlorosilane
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
    • H01L21/02205—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition
    • H01L21/02208—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
    • H01L21/02219—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and nitrogen
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02107—Forming insulating materials on a substrate
    • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
    • H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
    • H01L21/02263—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase
    • H01L21/02271—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition
    • H01L21/02274—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process deposition from the gas or vapour phase deposition by decomposition or reaction of gaseous or vapour phase compounds, i.e. chemical vapour deposition in the presence of a plasma [PECVD]

Definitions

  • the present invention is directed to the field of plasma enhanced low pressure chemical vapor deposition of silicon nitride films using aminosilanes, a range of ammonia or a relatively inert gas to improve the etch resistance and reduce the hydrogen concentration of the deposited silicon nitride.
  • a thin passive layer of a chemically inert dielectric material such as silicon nitride (Si 3 N 4 ) is essential. Thin layers of silicon nitride function as diffusion masks, oxidation barriers, trench isolation, intermetallic dielectric material with high dielectric breakdown voltages and passivation layers.
  • silicon nitride coatings in the fabrication of semiconductor devices are reported elsewhere, see Semiconductor and Process technology handbook, edited by Gary E. McGuire, Noyes Publication, New Jersey, (1988), pp 289-301; and Silicon Processing for the VLSI ERA, Wolf, Stanley, and Talbert, Richard N., Lattice Press, Sunset Beach, California (1990), pp 20-22, 327-330.
  • the present semiconductor industry standard silicon nitride growth method is by low pressure chemical vapor deposition ("LPCVD") in a hot wall reactor at >750°C using dichlorosilane and ammonia.
  • LPCVD low pressure chemical vapor deposition
  • Japanese Patent 6-132284 describes deposition of silicon nitride using organosilanes with a general formula (R 1 R 2 N) n SiH 4-n (where R 1 and R 2 range from H-, CH 3 -, C 2 H 5 - C 3 H 7 -, C 4 H 9 -) by a plasma enhanced chemical vapor deposition and thermal chemical vapor deposition in the presence of ammonia or nitrogen.
  • the precursors described here are tertiary amines and do not contain NH bonding as in the case of the present invention.
  • the deposition experiments were carried out in a single wafer reactor at 400°C at high pressures of 80-100 Torr.
  • the Si:N ratios in these films were 0.9 (Si:N ratios in Si 3 N 4 films is 0.75) with hydrogen content in the deposited films.
  • the butyl radical is in the form of isobutyl.
  • the major products in this process are aminochlorosilane, silicon nitride and ammonium chloride.
  • Formation of ammonium chloride is a major drawback of using Si-Cl containing precursors.
  • the formation of ammonium chloride leads to particle formation and deposition of ammonium chloride at the backend of the tube and in the plumbing lines and the pumping system. Processes which contain chlorine in the precursors result in NH 4 Cl formation. These processes require frequent cleaning and result in large down time of the reactors.
  • US Patent 5,874,368 teaches the use of bis(tertiarybutylamino)silane as a precursor to deposit silicon nitride using low pressure chemical vapor deposition at a temperature range of 500° to 800° C. Ammonia, nitrogen and argon are considered for reaction atmospheres, with ammonia present at greater than 1:1 ratios of the aminosilane.
  • US Patent 6,268,299 is directed to silicon nitride depositions using LPCVD, but makes the statement at col. 5, lines34-35; "Thus, the conventional PECVD process used to deposit nitride barrier films has a number of inherent disadvantages.”
  • US Patent 5,622,596 discloses at col. 3, lines 17-20 that silicon nitride stoichiometry can be related to silane and ammonia and nitrogen ratios in a plasma enhanced chemical vapor deposition (“PECVD”) process.
  • PECVD plasma enhanced chemical vapor deposition
  • the prior art has attempted to produce silicon nitride films at low temperatures, at high deposition rates and low hydrogen and carbon concentrations.
  • the low hydrogen is required because
  • the present invention has overcome the problems of the prior art with the use of aminosilanes in a PECVD process for the formation of silicon nitride which avoids the problems of the prior art, operates at low thermal conditions, avoids Si-C bonds to reduce carbon contamination of the resulting films, has low hydrogen concentrations, as well as avoiding chlorine contamination and operates at low pressures (20 mTorr - 2 Torr) in a manufacturable system as will be described in greater detail below.
  • the present invention is a process for the plasma enhanced chemical vapor deposition of high density silicon nitride on a substrate using an aminosilane and a reactant selected from the group consisting of nitrogen, argon, xenon, helium and high ratios of ammonia in relation to the aminosilane.
  • Figure 1 is a graph of Si-N absorbance wavenumbers vs. flow ratio of additive (NH3, N2 or He) to aminosilane, BTBAS, under the conditions shown in the graph, where lower wavenumber equates to higher density.
  • additive NH3, N2 or He
  • Figure 2 is FTIR spectra of silicon nitride films grown by PECVD using BTBAS, under the conditions shown in the graph
  • Figure 3 is FTIR spectra of silicon nitride films grown by PECVD using BIPAS, bis(isopropylamino)silane, under the conditions shown in the graph.
  • Figure 4 shows film stresses related to different additives used to deposit PECVD films using BIPAS.
  • Figure 5 compares etch rates of LPCVD and PECVD films as descibed in the graph.
  • VLSI Very Large Scale Integration
  • These deposited thin films can be of metals, semiconductors, or insulators.
  • the films may be thermally grown or deposited from the vapor phase using LPCVD.
  • VLSI technology requires very thin insulators for a variety of applications in both microprocessors and random-access memories device fabrication.
  • Silicon dioxide has been predominantly used as a dielectric material because of its ease of deposition and excellent properties at the SiO 2 /Si interface.
  • Silicon nitride has other advantages over silicon dioxide, some of these include impurity and dopant resistant diffusion barriers, high dielectric breakdown voltages, superior mechanical and inherent inertness of Si 3 N 4 .
  • the present invention is directed to a class of aminosilanes that deposit silicon nitride at unexpectedly low temperatures with superior uniformities and high densities under plasma enhanced chemical vapor deposition when an ammonia reactant is increased or replaced with nitrogen, helium, argon or xenon.
  • the aminosilane can include those structures set forth in Table 1 below.
  • BDEAES Bis(diethylamino)ethylsilane
  • BDEAS Bis(diethylamino)silane
  • the mono-, bis-, tris-, and tetrakis- structures are also included.
  • Bis(tertiarybutylamino)silane is particularly of interest and has the following formula: (t-C 4 H 9 NH) 2 Si(H) 2 .
  • the deposited films have superior uniformities and are free of ammonium chloride and chlorine contamination.
  • the bis(tertiarybutylamino)silane apparently has the property to deposit silicon nitride at 250-300°C below that of the dichlorosilane + ammonia process by LPCVD.
  • aminosilanes such as; bis(tertiarybutylamino)silane
  • N-Si bond may be attributable to the inherent property of the N-Si bond.
  • the presence of the N-H bond may facilitate labile ⁇ -hydride transfer to form diaminosilane.
  • the bis(tertiarybutylamino)silane and ammonia are allowed to react in the plasma to form precursors that result in silicon nitride depositions on a wafer at a wafer temperature of less than 500°C (preferably 420°C, but the temperature could be less or greater than this range). Reaction may occur either on the surface or very close to the wafer surface to deposit a thin silicon nitride film. If the reaction occurs in the gas phase (a homogeneous reaction) then clusters of silicon nitride are formed. Such cases are typical in silane and ammonia process. When the reaction occurs on the wafer surface, then the resulting films are of superior quality. Thus, one important requirement for a PECVD application is the degree to which heterogeneous reactions are favored over gas phase reactions.
  • the PECVD process can be grouped into a) a gas-phase process and b) a surface reaction process.
  • the gas phase phenomenon is the rate at which gases impinge on the substrate. This is modeled by the rate at which gases cross the boundary layer that separates the bulk regions of flowing gas and substrate surface. Such transport processes occur by gas-phase diffusion, which is proportional to the diffusivity of the gas and concentration gradient across the boundary layer.
  • Several surface processes can be important when the gases reach the hot surface, but the surface reaction, in general, can be modeled by a thermally activated phenomenon which proceeds at a rate which is a function of the frequency factor, the activation energy, and the temperature.
  • the surface reaction rate increases with increasing temperature.
  • the temperature may rise high enough so that the reaction rate exceeds the rate at which reactant species arrive at the surface. In such cases, the reaction cannot proceed any more rapidly than the rate at which reactant gases are supplied to the substrate by mass transport. This is referred to as a mass-transport limited deposition process.
  • the surface reaction rate is reduced, and eventually the concentration of reactants exceeds the rate at which they are consumed by the surface reaction process. Under such conditions the deposition rate is reaction rate limited.
  • the deposition is usually mass-transport limited, while at lower temperatures it is surface-reaction rate-limited.
  • the temperature at which the deposition condition moves from one of these growth regimes to the other is dependent on the activation energy of the reaction, and the gas flow conditions in the reactor. Thus, it is difficult to extrapolate process conditions or results from one pressure regime or temperature regime to another.
  • the temperature of the process is an important parameter. That is, uniform deposition rates throughout a reactor require conditions that maintain a constant reaction rate. This, in turn, implies that a constant temperature must exist everywhere on all wafer surfaces. On the other hand, under such conditions, the rate at which reactants reach the surface is not important, since their concentration does not limit the growth rate. Thus, it is not as critical that a reactor be designed to supply an equal flux of reactants to all locations of a wafer surface.
  • the vacuum system consisted of a rotary vane pump/roots blower combination and various traps.
  • the reactor pressure is controlled by a capacitance manometer feedback to a throttle valve controller.
  • Reactor loading was through a load-lock such that the reaction chamber was kept under vacuum at all times.
  • the present invention of a method of depositing etch-resistant, low hydrogen silicon nitride films on silicon wafers by using a aminosilane precursor with increasing quantities of ammonia or replacing ammonia with nitrogen, argon, xenon or helium has been demonstrated experimentally.
  • Bis(tertiarybutylamino)silane is a non-pyrophoric volatile liquid which is safer to handle than silane and dichlorosilane.
  • the deposition process is carried out at preferably 20mTorr-2Torr in the temperature range of 200 to 500°C, preferably 420°C, using vapors from bis(tertiarybutylamino)silane and ammonia.
  • an unreactive gas diluent such as nitrogen, helium, xenon or argon, can be used to dilute or replace the ammonia in order to achieve extremely high density silicon nitride films.
  • the molar feed ratio of ammonia to bis(tertiarybutylamino)silane is preferably in the range of 18:1 to 33:1
  • the process is performed in a cold wall PECVD reaction chamber.
  • the process steps are as follows:
  • Figure 1 is a graph of Si-N absorbance wavenumbers vs. flow ratio of additive (NH3, N2 or He) to aminosilane, BTBAS, under the conditions shown in the graph, where lower wavenumber equates to higher density.
  • additive NH3, N2 or He
  • Figure 2 is FTIR spectra of silicon nitride films grown by PECVD using BTBAS, under the conditions shown in the graph
  • BIS(isopropylamino)silane is also non-pyrophoric volatile liquid which is safer to handle than silane and dichlorosilane.
  • the process is identical to that in Example 1, except the precursor temperature is maintained at 40°C because of its higher vapor pressure than BTBAS.
  • the results of the PECVD depositions are shown in Figure 3 under conditions given in the graph. For comparison of hydrogen concentrations, LPCVD films have approximately 3 atomic percent hydrogen.
  • Figure 4 shows the film stress resulting from use of different additives. The stress may be modified by different combinations of additives.
  • Etch rates are a measure of the film composition and density of the as deposited silicon nitride films.
  • the data in Table 2 and Figure 5 demonstrates that the PECVD process of the present invention, using either increased ammonia reactant or replacing ammonia with an unreactive gas such as nitrogen or helium, and presumably, xenon or argon, results in very low etch rate silicon nitride films also.
  • Such apparently high-density silicon nitride films with increased resistance to etch are highly desirable in the electronic device fabrication industry because silicon nitride is frequently used as an etch stop against metal and oxide films, so that differential etch rates facilitate fabrication of metal-oxide-semiconductor composites with appropriate patterning.

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EP05018682A 2004-08-30 2005-08-29 Procédé de dépôt en phase vapeur de nitrure de silicium. Withdrawn EP1630249A3 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US10/929,755 US20060045986A1 (en) 2004-08-30 2004-08-30 Silicon nitride from aminosilane using PECVD

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EP1630249A2 true EP1630249A2 (fr) 2006-03-01
EP1630249A3 EP1630249A3 (fr) 2006-07-12

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EP (1) EP1630249A3 (fr)
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EP2192207A1 (fr) 2008-11-12 2010-06-02 Air Products And Chemicals, Inc. Précurseurs d'amino vinylsilane pour la deposition des films de SiN avec une contrainte de compression intrinsèque
EP2193541A1 (fr) * 2007-09-18 2010-06-09 L'AIR LIQUIDE, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Procédé de formation de films contenant du silicium
WO2013134661A1 (fr) * 2012-03-09 2013-09-12 Air Products And Chemicals, Inc. Matériaux barrière pour dispositifs d'affichage
US8889235B2 (en) 2009-05-13 2014-11-18 Air Products And Chemicals, Inc. Dielectric barrier deposition using nitrogen containing precursor
US20230357922A1 (en) * 2020-09-16 2023-11-09 Tokyo Electron Limited Sin film embedding method and film formation apparatus

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US20060172556A1 (en) * 2005-02-01 2006-08-03 Texas Instruments Incorporated Semiconductor device having a high carbon content strain inducing film and a method of manufacture therefor
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US20080207007A1 (en) 2007-02-27 2008-08-28 Air Products And Chemicals, Inc. Plasma Enhanced Cyclic Chemical Vapor Deposition of Silicon-Containing Films
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US7678715B2 (en) * 2007-12-21 2010-03-16 Applied Materials, Inc. Low wet etch rate silicon nitride film
US8129555B2 (en) * 2008-08-12 2012-03-06 Air Products And Chemicals, Inc. Precursors for depositing silicon-containing films and methods for making and using same
US8912353B2 (en) 2010-06-02 2014-12-16 Air Products And Chemicals, Inc. Organoaminosilane precursors and methods for depositing films comprising same
US8771807B2 (en) 2011-05-24 2014-07-08 Air Products And Chemicals, Inc. Organoaminosilane precursors and methods for making and using same
EP3929326A3 (fr) * 2011-06-03 2022-03-16 Versum Materials US, LLC Compositions et procédés pour le dépôt de films à teneur en silicium, dopés au carbone
WO2014015241A1 (fr) 2012-07-20 2014-01-23 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Précurseurs d'organosilane pour des applications faisant intervenir des films contenant du silicium dans des procédés ald/cvd
US9018108B2 (en) 2013-01-25 2015-04-28 Applied Materials, Inc. Low shrinkage dielectric films
US9382268B1 (en) 2013-07-19 2016-07-05 American Air Liquide, Inc. Sulfur containing organosilane precursors for ALD/CVD silicon-containing film applications
TW201509799A (zh) 2013-07-19 2015-03-16 Air Liquide 用於ａｌｄ／ｃｖｄ含矽薄膜應用之六配位含矽前驅物
KR102128589B1 (ko) * 2013-11-28 2020-06-30 에스피피 테크놀로지스 컴퍼니 리미티드 질화 실리콘막, 이의 제조방법, 및 이의 제조장치
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US10570513B2 (en) 2014-12-13 2020-02-25 American Air Liquide, Inc. Organosilane precursors for ALD/CVD silicon-containing film applications and methods of using the same
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EP2193541A1 (fr) * 2007-09-18 2010-06-09 L'AIR LIQUIDE, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Procédé de formation de films contenant du silicium
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US8580993B2 (en) 2008-11-12 2013-11-12 Air Products And Chemicals, Inc. Amino vinylsilane precursors for stressed SiN films
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